Method for simultaneously preparing two flavanone glycoside monomeric compounds by utilizing industrial chromatography technology
A technology of dihydroflavonoid glycosides and industrial chromatography, which is applied in the field of separation and purification of active ingredients of traditional Chinese medicine, can solve the problems that the separation process cannot realize real-time online monitoring, the purity and yield of ingredients are not high, and the purity of active ingredients is not high, so as to improve the quality of medicinal materials. The effect of utilization rate, short preparation process and simple operation
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Embodiment 1
[0033] Take Citrus aurantium, cut into decoction pieces or crush, add 4 times the amount of water, decoct 3 times, decoct and extract for 3 hours each time, combine the decoction liquid, filter, the filtrate passes through the treated non-polar macroporous resin, and then Elute with water and ethanol below 20% (19%) to remove impurities, then elute with 25% ethanol and 2% sodium hydroxide, collect the 25% ethanol eluate, concentrate under reduced pressure at 50-70°C to a relative density of about 1.40 The fluid extract, dried under reduced pressure at 80°C, and pulverized to obtain the total flavonoids extract of Citrus aurantium (see its HPLC chromatogram figure 1 ).
Embodiment 2
[0035] Take the citrus aurantium, cut into decoction pieces or crush, add 15 times the amount of water, decoct once, extract for 1 hour each time, combine the decoction liquid, filter, the filtrate passes through the treated non-polar macroporous resin, and then Elute with water and ethanol (15%) below 20% to remove impurities, then elute with 90% ethanol and 0.5% sodium hydroxide, collect the 90% ethanol eluate, concentrate under reduced pressure at 50-70°C to a relative density of about 1.20 The liquid extract was dried under reduced pressure at 60°C and crushed to obtain the total flavonoids extract of Citrus aurantium.
Embodiment 3
[0037] A kind of method that utilizes industrial chromatographic technique to prepare two kinds of dihydroflavonoid glycoside monomer compounds simultaneously (technical process sees figure 2 ), the dihydroflavone glycoside monomer compound is naringin and neohesperidin, comprising the following steps:
[0038] Get the total flavonoid glycosides extract of Fructus Fructus Fructus Aurantii gained in Example 1 (its HPLC chromatogram sees figure 1), wherein the content of naringin is about 15.0% (W / W), and the content of neohesperidin is about 20.0% (W / W), adding 5.0% (V / V) ethanol aqueous solution to dissolve it and prepare 105mg / ml concentration solution, filtered to obtain the sample solution.
[0039] Inject 100L of the sample solution into the industrial dynamic axial compression column system, the industrial chromatographic filler is UniSil30-100 (C18), ethanol: water: trifluoroacetic acid solution (35:65:0.3, V / V / V) as the eluent , the elution flow rate is 10.0CV / h, th...
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